5FBN

BTK kinase domain with inhibitor 1

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	ROTATING ANODE
Source details	RIGAKU MICROMAX-007 HF
Temperature [K]	100
Detector technology	IMAGE PLATE
Collection date	2010-09-01
Detector	RIGAKU RAXIS IV
Wavelength(s)	1.5418
Spacegroup name	P 1 21 1
Unit cell lengths	38.262, 71.475, 103.056
Unit cell angles	90.00, 90.68, 90.00

Refinement procedure

Resolution	103.050 - 1.800
R-factor	0.18232
Rwork	0.179
R-free	0.22596
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	not deposited inhouse model
RMSD bond length	0.015
RMSD bond angle	1.748
Data reduction software	MOSFLM
Data scaling software	SCALA
Phasing software	REFMAC
Refinement software	REFMAC (5.8.0135)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	36.000	1.900
High resolution limit [Å]	1.800	1.800
Rmerge	0.064	0.510
Number of reflections	48820
<I/σ(I)>	11.2	1.5
Completeness [%]	94.7	94.7
Redundancy	3.4	2.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	5.5	277	20% v/v PEG 20000 0.1M NaCl 0.1M Na MES pH 6.5 2.5 mM mM (S)-4-(8-amino-3-(1-(4-(dimethylamino)butanoyl)pyrrolidin-2-yl)imidazo[1,5-a]pyrazin-1-yl)-N-(thiazol-2-yl)benzamide 5.0 mM (R)-4-(8-amino-3-(1-(3-methyloxetane-3-carbonyl)piperidin-3-yl)imidazo[1,5-a]pyrazin-1-yl)-N-(4-(trifluoromethyl)pyridin-2-yl)benzamide